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The present work demonstrates preparation of magnetic nanoparticles by a novel method. Magnetic nanoparticles with potential for biomedical and environmental applications were obtained by homogeneous coprecipitation method sonochemically assisted. The effect of ultrasonic cavitation on changing the reaction environment was studied. The chemical reaction media used here was very similar to those used for Sono-Fenton process. The ultrasonic energy has driven the growth of particles; smaller diameter nanoparticles were obtained by applying a higher power. For the first time, it was demonstrated the iron oxide nanoparticles synthesis at pH lower than 6.

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In this study we report on successful production of two samples (BR15 and BR16) comprising magnetite (Fe 3 O 4) nanoparticles (~10 nm) surface-functionalized via hydrolysis and condensation of alkoxysilane agents, namely 3-aminopropyl-trimethoxisilane (APTS) and N-propyl-trimethoxisilane (NPTS). The as-produced samples were characterized using transmission electron microscopy (TEM), x-ray diffraction (XRD), magnetization measurements (5 K and 300 K hysteresis cycles and zero field-cooled/field-cooled measurements), and Mössbauer spectroscopy (77 and 297 K). The Mössbauer data supported the model picture of a core-shell magnetite-based system. This material system shows shell properties influenced by the surface-coating design, either APTS-coated (BR15) or APTS+NPTS-coated (sample BR16). Analyses of the Mössbauer spectra indicates that the APTS-coated sample presents Fe(III)-rich core and Fe(II)-rich shell with strong hyperfine field; whereas, the APTS+NPTS-coated sample leads to a mixture of two main nanostructures, one essentially surfaceterminated with APTS whereas the other surface-terminated with NPTS, both presenting weak hyperfine fields compared with the single surface-coated sample. Magnetization measurements support the core-shell picture built from the analyses of the Mössbauer data. Our findings emphasize the capability of the Mössbauer spectroscopy in assessing subtle differences in surface-functionalized iron-based core-shell nanostructures.